US2854494A - Process for purification of crystals - Google Patents

Process for purification of crystals Download PDF

Info

Publication number
US2854494A
US2854494A US494866A US49486655A US2854494A US 2854494 A US2854494 A US 2854494A US 494866 A US494866 A US 494866A US 49486655 A US49486655 A US 49486655A US 2854494 A US2854494 A US 2854494A
Authority
US
United States
Prior art keywords
zone
crystals
reflux
column
melt
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
US494866A
Other languages
English (en)
Inventor
Rosswell W Thomas
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Phillips Petroleum Co
Original Assignee
Phillips Petroleum Co
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority to DENDAT1192155D priority Critical patent/DE1192155B/de
Application filed by Phillips Petroleum Co filed Critical Phillips Petroleum Co
Priority to US494866A priority patent/US2854494A/en
Priority to GB6597/56A priority patent/GB807100A/en
Priority to FR1150173D priority patent/FR1150173A/fr
Priority to CH351255D priority patent/CH351255A/fr
Priority to FR1153982D priority patent/FR1153982A/fr
Application granted granted Critical
Publication of US2854494A publication Critical patent/US2854494A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Images

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/0004—Crystallisation cooling by heat exchange
    • B01D9/0013—Crystallisation cooling by heat exchange by indirect heat exchange
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Preparation or treatment thereof
    • A23L2/02—Non-alcoholic beverages; Dry compositions or concentrates therefor; Preparation or treatment thereof containing fruit or vegetable juices
    • A23L2/08—Concentrating or drying of juices
    • A23L2/12—Concentrating or drying of juices by freezing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/004—Fractional crystallisation; Fractionating or rectifying columns
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/005—Selection of auxiliary, e.g. for control of crystallisation nuclei, of crystal growth, of adherence to walls; Arrangements for introduction thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/0063—Control or regulation
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00—Purification; Separation; Use of additives
    • C07C7/14—Purification; Separation; Use of additives by crystallisation; Purification or separation of the crystals
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S585/00—Chemistry of hydrocarbon compounds
    • Y10S585/949—Miscellaneous considerations
    • Y10S585/953—Pulsed, sonic, or plasma process

Definitions

  • This invention relates to a process for the resolution of mixtures by crystallization. In one aspect, it relates to an improved apparatus for crystal purification.
  • Schmidt Re. 23,810 (1954) discloses a process and apparatus for purifying crystals, which process involves moving a mixture of crystals and adhering liquid through a liquid removal zone, a reflux Zone and a melting zone, removing liquid in said liquid removal zone, melting crystals in said melting zone, withdrawing part of the melt as product and forcing another part of the melt in a direction countercurrent to the movement of crystals in said reflux zone.
  • This process is generally applicable to the separation of at least one pure component from any mixture which is resolvable into its components by fractional crystallization.
  • the process can be used for the concentration of fruit juices, vegetable juices, and other.
  • the present invention provides a process and an apparatus for eifecting a separation of the type described at .higher throughput rates, improved stability and ease of operation, and improved heat distribution. In addition, products of high purity are obtainable over long periods of operation.
  • the solids are supplied continuously to said zone while the liquid is supplied intermittently.
  • a process which comprises moving a mass of solids, together with adhering liquid, through a liquid removal zone, then through a reflux zone and finally through a melting zone, withdrawing liquid in said liquid removal zone, melting at least part of said solids in said melting zone, removing part of the melt from said melting zone and forcing another part of said melt into said reflux zone in a direction countercurrent to the movement of solids therethrough, the improvement which comprises contacting the solids in said zones with an intermittent flow of reflux liquid simultaneously with the propulsion of said solids through said zones.
  • an apparatus comprising a purification chamber, liquid-solid separation means in said chamber, melting means positioned in one end of said chamber, means for moving solids to said separation means and thence toward said melting means, means for removing melt from said chamber, and means for removing liquid from said separation means, the improvement which comprises means for producing an intermittent fluid-flow in a di+ atent O 2,854,494 Patented Sept. 30, 1958 2 rection from said melting means toward said liquidsolid separation means.
  • a mass of crystals to be purified, together with accompanying liquid is passed through a purification chamber containing a filter which is integral with the wall of said chamber and positioned at an intermediate part thereof, then through a reflux zone toward a heating mean positioned in one end of the chamber, which heating means melts the crystals which arrive in the vicinity thereof.
  • the melt is withdrawn in part as purified product, and forced, in part, into the reflux zone toward the filter, and a pulsating back pressure is applied to the contents of the 'purification chamber by means of a reciprocating piston positioned in a cylinder which is in open communication with said chamber at the end in which said heating means is positioned.
  • the reciprocating motion of the piston can be produced by means which are well understood in the art, for example, by a mechanical crank attached to a motor or by an electric oscillator.
  • the back pressure is sufficient to produce a counterflow of liquid relative to the movement of the crystals.
  • Figure 1 illustrates one embodiment of this invention wherein pressure pulsations are produced by a reciproeating piston.
  • Figure 2 illustrates a modification of the apparatus of Figure 1.
  • Figure 3 illustrates a further modification wherein a flexible diaphragm is utilized.
  • the apparatus of Figure 1 comprises freezing or crystallizing means A, a filtering means B, a reflux zone C, a melting section D, and a pulsation-producing device E.
  • a feed mixture comprising two or more components, one of which is separable from the mixture by crystallization, enters the apparatus through inlet 2 and is forced by means of pump 3 into the chilling section A-of the main purification column.
  • the purification apparatus is composed of a cylindrical shell 4, to which is attached a cooling section which comprises a cylindrical shell 5.
  • the shells 5 and 5 can be constructed of ordinary metal pipe and can be welded together at any desired angle, as indicated in the drawing; or they can be connected by flanges or by threads. Alternatively, they can be one single length of pipe which can be built in the form of an elbow at any desired angle. The particular angle shown in the drawing can vary within a very broad range or the entire apparatus can be straight.
  • Crystallization section A comprises, in addition to shell 5, a cooling jacket 8 having inlet 9 and outlet 10. Positioned within the crystallization section is an agitating or scraping means 11, which is designed to prevent the accumulation of solid material on the heat exchange surface.
  • Scrapers 11 are suitablyconstructed of strips of metal or other suitable materials known in the art. They can be fabricated in the form of a helix, as indicated in the drawing, or can be straight. Any suitable number of scrapers 11 can be provided. They are mounted on a rotatable shaft 12 by means of members 13. Shaft 12 is axially positioned in shell 5 and is connected to any suitable source of power for rotat- 'of any desired type known in the art.
  • Shaft 12 is suitably sealed in end member 6 by means of a packing gland of any desired type known in the art.
  • Suitable cooling of the feed which enters shell can be provided byaddinga coolant through inlet 9 and withdrawing thecoolant through outlet 10.
  • Suflicient cooling in section A is" provided so ably positioned within the purification column at a point by thermocouple 29 to an air pressure which is utilized that a predetermined amount of solid crystals is produced,-as subsequently discussed herein.
  • the resulting crystal mass passes through purification chamber 4. and into filter section B. 7
  • the feed pump 3 is generally suitable for forcing the crystal mixture through the purifica-' tion column.
  • othermeans for propelling the mixture through the purification zone can beprovided, as shown in the cited Schmidt reissue patent. Where such means, for example, a piston, is provided, it can be positioned upstream from section A or intermediate the chilling section A'and purification section 4, or other suitable arrangements can be provided by those skilled in the art.
  • Filtration section B comprises a suitable filter medium 14 and an external shell 15, the latter being provided with anoutlet pipe 16 for filtrate.
  • Filter medium 14 can be For example, it can comprise a metallic screen, a sintered perforate metal member or a perforate metal member supporting a filter cloth. In any event, it is desirable that the filter member 14 be positioned integrally with respect to the shell 4.
  • Filtrate produced in filter zone B is removed from the system through outlet 16.
  • Heater 17 can be in -the formof an electrical heater or a heat transfer coil through which a suitably heated fluid is pumped. Part of the melt produced by heater 17 is withdrawn through outlet pipe 18 as a purified product of the process. The remainder of the melt is forced back through reflux zone C to form reflux which effects crystal purification, the
  • an internalheater 17 an external heater, for example, a heating jacket encompassing section D and provided with means for circulating a heating fluid therethrough, can be used, if desired.
  • the pulsation-producing member E comprises a cylinder 19 which is suitably attached to closure member 7 as, for example, by welding, and closure means 20, together with a reciprocatable piston 21.
  • Piston 21 is suitably sealed in cylinder 19, for example, by means of rings 22, to prevent the leakage of melt from the purification.
  • Reciprocationof piston 21 is produced, for example, by an electric motor 23, a belt 24, a crank means 25, and connecting rods 26, which can be sealed in closure member 20 by means of a packing gland.
  • 'An outlet 27 is provided in closure member 20 to facilitate the reciprocation of piston 21 and can be connected to means, notshown, for recovery of any material which might escape from column 4 in case of failure of rings 22.
  • piston 21 is reciprocated at a suitable rate, which is subsequently discussed herein, so that a pulsating pressure is exerted on the melt reflux which is intermittently forced ack, countercurrently with respect to the crystal mass, through reflux zone C.
  • melt outlet 18 is positioned a check valve 28 to prevent the back flow 0f withdrawn melt into the crystal purification column.
  • a temperature recorder-controller designated in the drawto open or close valve 30.
  • the temperature recordercontroller is suitably so adjusted that an undesirably rapid advance of crystals through reflux zone C results in a predetermined low temperature which is measured by thermocouple 29, which operates through the temperature recorder-controller to throttle valve 30 and decrease the rate of withdrawal of melt.
  • An undesirably slow advance of crystals through the purification column produces the opposite effect.
  • Cycle control device 31 of known design, which is operatively'connected with motor 23 so that an electrical pulse is produced in synchronism with piston 21.
  • the cycle control 31 can be so adjusted that, on the compression stroke of piston 21, an otherwise closed solenoid valve 32 is opened, resulting in the removal of filtrate from the purification column only on the compression stroke of piston 21.
  • check valve 33 in filtrate withdrawal line 16.
  • a similar arrangement can be effected in connection with the withdrawal of melt through outlet 18. However, it is preferred, in such a case, that the melt withdrawal cease during the compression strokeof the piston. Means for producing this result are not shown in the drawing.
  • Cycle control means 31 can, for example, be operatively connected to crank 25 or connecting rods 26. It can include an electrical make-and-break device, such devices being well known in the art.
  • a suitable, and often preferred, arrangement is to utilize bypass 34, solenoid valve 32 and/or check valve 33 being closed and by-passed.
  • bypass 34 solenoid valve 32 and/or check valve 33 being closed and by-passed.
  • PIC pressure indicator-controller
  • This instrument is of a type well known in the art and converts a back-pressure in the liquid withdrawal line 16 to an air pressure, which suitably throttles motor valve 35 to maintain a desired back-pressure in line 16.
  • a similar instrument arrangement can be utilized ingas TRC, is provided and is connected to asuitable in connection with valve 36 in melt withdrawal line 18.
  • the cylinder 20 is spaced from the cylinder 4 and is connected therewith by means of an open conduit 40.
  • the piston 20 is separated from the contents of thepurification column by means of an intermediate fluid which is supplied through valved conduit 50.
  • the piston acts-directly upon the intermediate fluid and, in turn,-produces a pulsation of a flexible diaphragm 51, which is suitably sealed within a chamber 52.
  • the intermediate fluid can be any noneorros'ive fluid. It is :preferabl'y'a liquid, such as a vegetable oil, which is inert with respect to the materials being separated in column 4 and which is readily a" mineral lubricating oil or and chamber 52.
  • diaphragm 51 can be actuated pneumatically, or by means of a direct, reciproeating, mechanical linkage attached to the"diaphragm, or electrically, as by means of a solenoid, or by any other desiredmeans for producing a reciprocating fiex-ure.
  • the diaphragm can be placed in end'member 7, e. g., concentrically therewith, or 'can replaceend member 7, the melt being withdrawn from a side outlet. Further, the diaphragm 'can'be sonically or supersonically, or even subsonically, vibrated. 1
  • purification chamber 4 is shown positioned horizontally, it can beoperated in other positions; for example, it can be maintained in a vertical 'position'with cylinder and piston 21 at the top. This arrangement utilizes gravity as an aid to the flow of reflux.
  • an additional piston can be'utilized for propelling the crystals through'thecrystallization column, I have found that sucha' device is ordinarily unnecessary,'suitable propulsion beingprovided by a feed pump 3, especially when the purification column is horizontal or nearly horizontal.
  • scope of this invention to utilize two pistons, one to propel the crystals through the purification column and the other to produce'a pulsating reflux stream.
  • Thelatter piston is ordinarily operated at a frequency greater than that of the former, so that during a sustained movement of solids within a given time interval, an intermittent counterflow of reflux liquid is simultaneously effected.
  • A- further suitable modification of the invention can be provided by positioning in reflux zone C a heat-transfer grid of the type shown in the copending application of T. A. Tarr, Serial No. 477,099, filed December 22, 1954. It has been found that certain ranges of frequency of pulsation of the back-pressure applied according to this invention produces results superior to certain other ranges of frequency. In the separation of para-xylene from its isomers, improved results are obtainable at a frequency as low as 15 pulsations per minute or as high as 200 pulsations per minute. However, outstanding results are obtained at from 50 to 165 pulsations per minute. Highly superior results are obtained in the range from 125 to 1 50 pulsations per minute. It has been found that within the preferred range the" operation of the purification column is greatly stabilized and the movement of material It is, however, within the,
  • phase equilibrium is greatly facilitated by the use of pulsating back-pressure and reflux flow according to this invention.
  • a critical lower limit of frequency exists at about 50 pulsations per minute in the purification of para-xylene. Broadly, however, the invention is not so limited.
  • the dimensions of the cylinder and piston used to pro prise the back-pressure pulsation can vary over a rather wide range. It has been found that when a purification column 6 inches in diameter is used in conjunction with a two inch diameter piston for the separation of paraxylene from its isomers, the piston stroke can be in the range /2 to 2 /2 inches, preferably /1 to 2 inches, and it has been found that a 1-inch stroke appears to produce optimum results in terms of ease and stability of opera tion. Optimum dimensions in any particular case can readily be determined by trial by those skilled in the art. It is to be understood that the dimensions, configurations, and frequencies stated above are not necessarily optimum for every material to be purified.
  • back-pressure within the purification column is preferably applied by the piston or other pulsator in a'regular or periodic or pulsating manner
  • an irregular or non-periodic increase of back-pressure is within the scope of the invention.
  • electrical, pneumatic or hydraulic actuation of the pulsating mechanism can be utilized in place of purely mechanical actuation.
  • the first unit can be operated with or without the use of pulsating back-pressure, a pulsating backpressure being used in the second unit. More than two such units can be used in series. Alternatively, the preliminary concentration can be accomplished by crystallization and subsequent filtration, although this method is not necessarily equivalent to the use of two or more pulsator-equipped units in series as previously described.
  • temperature recorder-controller was provided for measur- 8 ing the. temperature at the electri l heater within the column and controlling the product withdrawal rate, in
  • Chiller outlet Thepurificationi-unit utilized in these examples was of the type illustrated in Figure 1. was constructed of flangedsteel pipe 6 inches 111 diameter and approximately 2% feet in length, the column being 10 'withthe electrical heater. Thus, if crystals melted upof flangesat an angle of ,8 40f with,the h,orizonta 1
  • the chiller was providcdwith a; jacket through which coolant l5 filtrate withdrawalline was synchronized with the 2-inch was circulated, Within thechi-llerwas a scraper of the which was connected a 2-inch diameter cylinder provided with a piston, as illustrated in Figure 1;
  • the 2-inch piston was driven by means of a mechanical linkage with Period oioperation,
  • Table III OPERATING DATA [ti-inch. diameter, horizontal, pulsed column 60 percent p-xylene feed-fractional crystallization] Temperatures, F. Pressures, p. s. i. g. Pulse piston Rates, G. P. H. Stream composition, mol percent p-xylene Duratign of Heat, watts run, r.
  • EXAMPLE III This example illustrates the effect of pulsation frequency on the purification of para-xylene according to this invention.
  • the purification column was vertically positioned EXAMPLE II and had a length of approximately 26 inches and a di- 35 ameter of approximately 5% inches.
  • the filter was 7 d In a systen 9 s lf? ig u l f f inches long and provided 46 square inches of filtration ata were 0 s Owmg e res ts varymg Ce am area.
  • the purification column was connected, by means other process variables.
  • Mother liquor rate was controlled by instrument, based on the chiller outlet pressure.
  • creasing the frequency to 32 cycles per minute resulted in a further increase in purity. Further increase to 66 and to 99 cycles per minute, and a further increase to 127 cycles per minute, produced much improved results.
  • Benzene 80 5 n-Hexane 69 94 n-Heptane, 98. 52 go. 5 Carbon tetrachloride. 77 22. 8 Acrylonitrile 79 82 Ethyl alcohol 78. 5 117. 3 2,2-dlmethylpentane 79 125 3,3-dlmethylpentane 86 Methyl ethyl ketone 79. 6 86. 4 Methyl proplonate 79. 9 87. 5 Methyl acrylate--. 80. 5 1,3-cyc1ohexadiene-. 80. 5 98 2,4-dimethylpentane 80. 8 123.
  • Benzene can be'separated from a benzene-n-hexane or a benzene-n-heptane mixture in which the benzene is present in an amount greater than the eutectic concentration.
  • paraxylene can be readily separated from a mixture of paraand meta-xylenes or from para-, meta-, or ortho-xylenes.
  • Benzene can also be separated from a mixture thereof with toluene and/or aniline.
  • Multi-component mixtures which can be effectively resolved so as to recover one or more of the components in substantially pure form include mixtures of at least two of 2,2-dimethylpentane, 2,4-dimethylpentane,'2,2,3-trimethylbutane, methyl cyclohexane, and 2,2,4-trimethylpentane, and mixtures of at least two of carbon tetrachloride, chloroform, and acetone.
  • the invention is also applicable to the separation of individual components from a mixture of cymenes.
  • This invention can also be utilized to purify crude naphthalene, hydroquinone (1,4-benzenediol), paracresol, para-dichlorobenzene, and'such materials as high melting Waxes, fatty acids, and high molecular weight normal paraffins.
  • the invention can also be used to resolve a mixture comprising anthracene, phenanthrene, and carbazole.
  • the invention can be used to separate durene (1,2,4,S-tetramethylbenzene) from other C aromatics.
  • the impure material is raised to a temperature at which only a portion of the mixture is in a crystalline state, and the resulting slurry is handled at such a temperature that operation is as described in connection with materials which crystallize at lower'temperatures.
  • the invention is also applicable to the concentration of food products.
  • the process consists generally of the removal of water, in the form of ice crystals, from such products.
  • One special class of foods which can be concentrated in this manner is that of fruit juices, such as grape, pineapple, watermelon, apple, orange, lemon, lime, tangerine, grapefruit, and the like.
  • Beverages such as milk, wine, beer, coffee, tea, and various liquors, can also be concentrated in such a process.
  • the process is also applicable to theconcentration of vegetable juices.
  • a process which compriseschilling a fruit juice to obtain a confined mass of ice crystals, passing said crystals and adhering liquor through a' filtration zone, removing liquor from said filtration zone as a product of the process, passing remaining solids through a reflux zone.
  • a process for recovering para-xylene from a mixture comprising at least one other xylene and ethyl benzone comprises cooling the mixture to obtain a solids content in the range 25 to 30 weight percent, said solids being p'reponderantly para-xylene crystals, passing the resulting mixture of crystals and liquid through a filtration zone, removing liquid from said filtration zone, passing the crystals, in the form of a confined mass of contiguous crystals with adhering mother liquor, through a reflux zone in counter-current contact with reflux liquid produced as subsequently described, passing the crystals into a melting zone and therein melting said crystals, withdrawing purified molten para-xylene as a product of the process, passing the remainder of the molten material, in the form of a pulsating stream, into said reflux zone in a direction counter-current to the movement of crystals therethrough, and directly applying a pulsating back-pressure substantially only tosaid molten material at a frequency in the range
  • Attest KARL H. AXLINE, ROBERT C. WATSON, Attesting Ofioer. Commz'ssz'oner of Patents.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Thermal Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Water Supply & Treatment (AREA)
  • Nutrition Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Analytical Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
US494866A 1955-03-17 1955-03-17 Process for purification of crystals Expired - Lifetime US2854494A (en)

Priority Applications (6)

Application Number Priority Date Filing Date Title
DENDAT1192155D DE1192155B (de) 1955-03-17 Verfahren zum kontinuierlichen Reinigen von Kristallsuspensionen
US494866A US2854494A (en) 1955-03-17 1955-03-17 Process for purification of crystals
GB6597/56A GB807100A (en) 1955-03-17 1956-03-02 Improvements in process and apparatus for purification of crystals
FR1150173D FR1150173A (fr) 1955-03-17 1956-03-16 Perfectionnements à un procédé et à un appareil pour la purification des cristaux
CH351255D CH351255A (fr) 1955-03-17 1956-03-16 Procédé et appareil pour la résolution de mélanges par cristallisation
FR1153982D FR1153982A (fr) 1955-03-17 1956-06-08 Procédé de purification par cristallisation

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US494866A US2854494A (en) 1955-03-17 1955-03-17 Process for purification of crystals

Publications (1)

Publication Number Publication Date
US2854494A true US2854494A (en) 1958-09-30

Family

ID=23966303

Family Applications (1)

Application Number Title Priority Date Filing Date
US494866A Expired - Lifetime US2854494A (en) 1955-03-17 1955-03-17 Process for purification of crystals

Country Status (5)

Country Link
US (1) US2854494A (fr)
CH (1) CH351255A (fr)
DE (1) DE1192155B (fr)
FR (2) FR1150173A (fr)
GB (1) GB807100A (fr)

Cited By (42)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2913344A (en) * 1955-11-10 1959-11-17 Phillips Petroleum Co Process and apparatus for purification of crystals
US2945903A (en) * 1956-12-26 1960-07-19 Phillips Petroleum Co Fractional crystallization process and apparatus
US2983589A (en) * 1956-09-24 1961-05-09 Phillips Petroleum Co Process for the purification of crystals
US3017752A (en) * 1959-08-28 1962-01-23 Phillips Petroleum Co Desalting sea water
US3050952A (en) * 1960-10-05 1962-08-28 Phillips Petroleum Co Separation by crystallization
US3119771A (en) * 1960-07-27 1964-01-28 Phillips Petroleum Co Desalting aqueous salt solutions by the formation of hydrocarbon hydrates and the purification thereof
US3150500A (en) * 1963-07-05 1964-09-29 Phillips Petroleum Co Purification of crystals
US3178900A (en) * 1963-08-05 1965-04-20 James E Saunders Apparatus for the removal of salt from sea water
US3190450A (en) * 1962-08-06 1965-06-22 Phillips Petroleum Co Filter for a crystal purification column
US3193395A (en) * 1962-05-04 1965-07-06 Phillips Petroleum Co Concentration of beer by crystallization
US3212282A (en) * 1962-07-02 1965-10-19 Phillips Petroleum Co Fractional crystallization control system
US3219722A (en) * 1961-12-05 1965-11-23 Chevron Res Cyclic crystallization process
US3218818A (en) * 1963-04-01 1965-11-23 Phillips Petroleum Co Fractional crystallization control system
US3222880A (en) * 1963-01-03 1965-12-14 Phillips Petroleum Co Fractional crystallization control system
US3240024A (en) * 1961-11-08 1966-03-15 Carrier Corp Freeze crystallization separation systems
US3240025A (en) * 1962-07-05 1966-03-15 Phillips Petroleum Co Concentrating beer containing carbon dioxide by crystallization at elevated pressure
US3243968A (en) * 1962-05-17 1966-04-05 Phillips Petroleum Co Fractional crystallization
US3261170A (en) * 1963-05-10 1966-07-19 Phillips Petroleum Co Multi-stage crystallization process and apparatus
US3285027A (en) * 1964-11-25 1966-11-15 Phillips Petroleum Co Pulsed crystal reflux with a minimal melt
US3285022A (en) * 1963-01-08 1966-11-15 John W Pike Concentration of extracts by freezing
US3323920A (en) * 1963-02-25 1967-06-06 Phillips Petroleum Co Concentration of beer by crystallization and distillation
US3354083A (en) * 1964-02-20 1967-11-21 Dept Of Chemical Engineering Separation of fresh water from aqueous solutions
US3402047A (en) * 1964-08-14 1968-09-17 Phillips Petroleum Co Crystallization separation and purification utilizing fresh feed to reslurry crystals
US3403029A (en) * 1964-11-06 1968-09-24 Phillips Petroleum Co Reconstituted beer process using fractional crystallization
US3404006A (en) * 1964-08-31 1968-10-01 Phillips Petroleum Co Wine preparation by fermenting a juice, concentrating the fermented product, and optionally fortifying the concentrate
DE1286507B (de) * 1962-05-14 1969-01-09 Phillips Petroleum Co Verfahren zum Konzentrieren eines aus mehreren Bestandteilen bestehenden fluessigen Materials
DE1295516B (de) * 1965-10-07 1969-05-22 Mannesmann Ag Verfahren zum Trennen einer Loesung in eine an einer Komponente ab- und eine daran angereicherte Loesung
DE1298079B (de) * 1962-06-28 1969-06-26 Phillips Petroleum Co Verfahren zum Trennen von Kristallen von Mutterlauge beim fraktionierten Kristallisieren
US3487652A (en) * 1966-08-22 1970-01-06 Phillips Petroleum Co Crystal separation and purification
US3630685A (en) * 1968-11-15 1971-12-28 Herman Schildknecht Method for the transportation of crystals and melt
US3872009A (en) * 1971-06-25 1975-03-18 Henricus Alexis Corne Thijssen Apparatus for the separation and treatment of solid particles from a liquid suspension
US4597768A (en) * 1982-06-22 1986-07-01 Nederlandse Centrale Organisatie Voor Toegepast Natuurwetenschappelijk Onderzoek Method for treatment in counter current of suspended particles with a liquid
US4735781A (en) * 1982-06-22 1988-04-05 Nederlandse Centrale Organisatie Voor Toegepast Natuurwetenschappelijk Onderzoek Juliana Van Stolberglaan Apparatus for concentrating a suspension
US5090965A (en) * 1988-08-12 1992-02-25 Bayer Aktiengesellschaft Process for the separation of substances by cooling crystallization
WO2001013050A1 (fr) * 1999-08-13 2001-02-22 Cheng Sing Wang Systeme pour faire monter la temperature de chauffage
EP1295628A1 (fr) * 2001-09-19 2003-03-26 Niro Process Technology B.V. Colonne de lavage hydraulique et procédé de séparation de solides d' une suspension
US20040256319A1 (en) * 2001-11-15 2004-12-23 Ulrich Hammon Method for performing the purifying separation of crystals out their suspension in a mother liquor
US20050056599A1 (en) * 2003-09-16 2005-03-17 Wilsak Richard A. Solid-liquid separation process
US20100041936A1 (en) * 2008-08-14 2010-02-18 Bp Corporation North America Inc. Melt-crystallization separation and purification process
US8962906B2 (en) 2006-03-21 2015-02-24 Bp Corporation North America Inc. Apparatus and process for the separation of solids and liquids
CN113545489A (zh) * 2021-07-02 2021-10-26 新疆农业大学 一种制备果蔬澄清汁的装置和方法
CN115090116A (zh) * 2022-07-26 2022-09-23 河南羲和化工科技有限公司 一种依西美坦中间体的提纯装置

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1292635B (de) * 1958-10-24 1969-04-17 Fischbeck Verfahren zur kontinuierlichen Trennung von Mischungsbestandteilen
AT389122B (de) * 1988-05-17 1989-10-25 Verfahren zum herstellen von konzentraten aus wasserhaeltigen fluessigkeiten

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2540977A (en) * 1945-01-02 1951-02-06 Phillips Petroleum Co Continuous fractional crystallization process
US2598449A (en) * 1947-08-13 1952-05-27 Midland Tar Distillers Ltd Purification of naphthalene
US2615794A (en) * 1950-06-26 1952-10-28 Phillips Petroleum Co Crystallization apparatus
US2617274A (en) * 1949-02-09 1952-11-11 Joachim Schmidt Process and apparatus for concentrating solutions
US2622114A (en) * 1948-12-31 1952-12-16 Phillips Petroleum Co Fractional crystallization process and apparatus
US2683178A (en) * 1950-07-28 1954-07-06 Phillips Petroleum Co Crystal purification process and apparatus
US2724508A (en) * 1954-05-26 1955-11-22 Sun Oil Co Separator for solid-liquid slurry

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2540977A (en) * 1945-01-02 1951-02-06 Phillips Petroleum Co Continuous fractional crystallization process
US2598449A (en) * 1947-08-13 1952-05-27 Midland Tar Distillers Ltd Purification of naphthalene
US2622114A (en) * 1948-12-31 1952-12-16 Phillips Petroleum Co Fractional crystallization process and apparatus
US2617274A (en) * 1949-02-09 1952-11-11 Joachim Schmidt Process and apparatus for concentrating solutions
US2615794A (en) * 1950-06-26 1952-10-28 Phillips Petroleum Co Crystallization apparatus
US2683178A (en) * 1950-07-28 1954-07-06 Phillips Petroleum Co Crystal purification process and apparatus
US2724508A (en) * 1954-05-26 1955-11-22 Sun Oil Co Separator for solid-liquid slurry

Cited By (50)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2913344A (en) * 1955-11-10 1959-11-17 Phillips Petroleum Co Process and apparatus for purification of crystals
US2983589A (en) * 1956-09-24 1961-05-09 Phillips Petroleum Co Process for the purification of crystals
US2945903A (en) * 1956-12-26 1960-07-19 Phillips Petroleum Co Fractional crystallization process and apparatus
US3017752A (en) * 1959-08-28 1962-01-23 Phillips Petroleum Co Desalting sea water
US3119771A (en) * 1960-07-27 1964-01-28 Phillips Petroleum Co Desalting aqueous salt solutions by the formation of hydrocarbon hydrates and the purification thereof
US3050952A (en) * 1960-10-05 1962-08-28 Phillips Petroleum Co Separation by crystallization
US3240024A (en) * 1961-11-08 1966-03-15 Carrier Corp Freeze crystallization separation systems
US3219722A (en) * 1961-12-05 1965-11-23 Chevron Res Cyclic crystallization process
US3193395A (en) * 1962-05-04 1965-07-06 Phillips Petroleum Co Concentration of beer by crystallization
DE1286507B (de) * 1962-05-14 1969-01-09 Phillips Petroleum Co Verfahren zum Konzentrieren eines aus mehreren Bestandteilen bestehenden fluessigen Materials
US3243968A (en) * 1962-05-17 1966-04-05 Phillips Petroleum Co Fractional crystallization
DE1298079B (de) * 1962-06-28 1969-06-26 Phillips Petroleum Co Verfahren zum Trennen von Kristallen von Mutterlauge beim fraktionierten Kristallisieren
US3212282A (en) * 1962-07-02 1965-10-19 Phillips Petroleum Co Fractional crystallization control system
US3240025A (en) * 1962-07-05 1966-03-15 Phillips Petroleum Co Concentrating beer containing carbon dioxide by crystallization at elevated pressure
DE1265128B (de) * 1962-07-05 1968-04-04 Phillips Petroleum Co Verfahren zum Konzentrieren von Loesungen durch Kristallisation
US3190450A (en) * 1962-08-06 1965-06-22 Phillips Petroleum Co Filter for a crystal purification column
US3222880A (en) * 1963-01-03 1965-12-14 Phillips Petroleum Co Fractional crystallization control system
US3285022A (en) * 1963-01-08 1966-11-15 John W Pike Concentration of extracts by freezing
US3323920A (en) * 1963-02-25 1967-06-06 Phillips Petroleum Co Concentration of beer by crystallization and distillation
US3218818A (en) * 1963-04-01 1965-11-23 Phillips Petroleum Co Fractional crystallization control system
US3261170A (en) * 1963-05-10 1966-07-19 Phillips Petroleum Co Multi-stage crystallization process and apparatus
US3150500A (en) * 1963-07-05 1964-09-29 Phillips Petroleum Co Purification of crystals
US3178900A (en) * 1963-08-05 1965-04-20 James E Saunders Apparatus for the removal of salt from sea water
US3354083A (en) * 1964-02-20 1967-11-21 Dept Of Chemical Engineering Separation of fresh water from aqueous solutions
US3402047A (en) * 1964-08-14 1968-09-17 Phillips Petroleum Co Crystallization separation and purification utilizing fresh feed to reslurry crystals
US3404006A (en) * 1964-08-31 1968-10-01 Phillips Petroleum Co Wine preparation by fermenting a juice, concentrating the fermented product, and optionally fortifying the concentrate
US3403029A (en) * 1964-11-06 1968-09-24 Phillips Petroleum Co Reconstituted beer process using fractional crystallization
US3285027A (en) * 1964-11-25 1966-11-15 Phillips Petroleum Co Pulsed crystal reflux with a minimal melt
DE1295516B (de) * 1965-10-07 1969-05-22 Mannesmann Ag Verfahren zum Trennen einer Loesung in eine an einer Komponente ab- und eine daran angereicherte Loesung
US3487652A (en) * 1966-08-22 1970-01-06 Phillips Petroleum Co Crystal separation and purification
US3630685A (en) * 1968-11-15 1971-12-28 Herman Schildknecht Method for the transportation of crystals and melt
US3872009A (en) * 1971-06-25 1975-03-18 Henricus Alexis Corne Thijssen Apparatus for the separation and treatment of solid particles from a liquid suspension
US4597768A (en) * 1982-06-22 1986-07-01 Nederlandse Centrale Organisatie Voor Toegepast Natuurwetenschappelijk Onderzoek Method for treatment in counter current of suspended particles with a liquid
US4735781A (en) * 1982-06-22 1988-04-05 Nederlandse Centrale Organisatie Voor Toegepast Natuurwetenschappelijk Onderzoek Juliana Van Stolberglaan Apparatus for concentrating a suspension
US4743434A (en) * 1982-06-22 1988-05-10 Nederlandsche Centrale Organisatie Voor Toegepast Natuurwetenschappelijk Onderzoek Apparatus for treatment of suspended particles with a liquid in countercurrent
US5090965A (en) * 1988-08-12 1992-02-25 Bayer Aktiengesellschaft Process for the separation of substances by cooling crystallization
WO2001013050A1 (fr) * 1999-08-13 2001-02-22 Cheng Sing Wang Systeme pour faire monter la temperature de chauffage
EP1295628A1 (fr) * 2001-09-19 2003-03-26 Niro Process Technology B.V. Colonne de lavage hydraulique et procédé de séparation de solides d' une suspension
US20040256319A1 (en) * 2001-11-15 2004-12-23 Ulrich Hammon Method for performing the purifying separation of crystals out their suspension in a mother liquor
US7540884B2 (en) 2001-11-15 2009-06-02 Basf Aktiengesellschaft Method for performing the purifying separation of crystals out their suspension in a mother liquor
US20050056599A1 (en) * 2003-09-16 2005-03-17 Wilsak Richard A. Solid-liquid separation process
EP1842577A1 (fr) * 2003-09-16 2007-10-10 BP Corporation North America Inc. Procédé de séparation solide-liquide
US8211319B2 (en) 2003-09-16 2012-07-03 Bp Corporation North America Inc. Solid-liquid separation process
US8962906B2 (en) 2006-03-21 2015-02-24 Bp Corporation North America Inc. Apparatus and process for the separation of solids and liquids
US20100041936A1 (en) * 2008-08-14 2010-02-18 Bp Corporation North America Inc. Melt-crystallization separation and purification process
US8530716B2 (en) 2008-08-14 2013-09-10 Bp Corporation North America Inc. Melt-crystallization separation and purification process
CN113545489A (zh) * 2021-07-02 2021-10-26 新疆农业大学 一种制备果蔬澄清汁的装置和方法
CN113545489B (zh) * 2021-07-02 2023-08-22 新疆农业大学 一种制备果蔬澄清汁的装置和方法
CN115090116A (zh) * 2022-07-26 2022-09-23 河南羲和化工科技有限公司 一种依西美坦中间体的提纯装置
CN115090116B (zh) * 2022-07-26 2024-04-09 河南羲和化工科技有限公司 一种依西美坦中间体的提纯装置

Also Published As

Publication number Publication date
CH351255A (fr) 1961-01-15
FR1153982A (fr) 1958-03-31
DE1192155B (de) 1965-05-06
FR1150173A (fr) 1958-01-08
GB807100A (en) 1959-01-07

Similar Documents

Publication Publication Date Title
US2854494A (en) Process for purification of crystals
US2747001A (en) Crystal purification process
US2765921A (en) Crystal purification process and apparatus
US2780663A (en) Fractional crystallization and crystal washing
US2815364A (en) Fractional crystallization process and apparatus
US2835598A (en) Separation by crystallization
US3261170A (en) Multi-stage crystallization process and apparatus
US2800411A (en) Crystal purification apparatus and process
US3093649A (en) Fractional crystallization process
US2895835A (en) Separation by crystallization
US2885431A (en) Separation by crystallization
US2874199A (en) Fractional crystallization process and apparatus
US2981773A (en) Separation by crystallization
US2919991A (en) Method of controlling crystal purification process and apparatus therefor
US3050952A (en) Separation by crystallization
US2891099A (en) Fractional crystallization process and apparatus
US3402047A (en) Crystallization separation and purification utilizing fresh feed to reslurry crystals
US2823242A (en) Process and apparatus for crystal purification and separation
US2890962A (en) Process and apparatus for purification of crystals
US2809884A (en) Apparatus for separation by crystallization
US3092673A (en) Method and apparatus for crystal purification
US3190450A (en) Filter for a crystal purification column
US3212281A (en) Fractional crystallization
US3267686A (en) Fractional crystallization having a liquor withdrawal responsive to a pressure differential
US2913344A (en) Process and apparatus for purification of crystals